CN102274713B - Method for preparing benzene adsorbing material by utilizing discarded activated aluminum oxide - Google Patents
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- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 title claims abstract description 63
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 14
- 239000000463 material Substances 0.000 title claims abstract description 13
- 239000002699 waste material Substances 0.000 claims abstract description 39
- 238000001179 sorption measurement Methods 0.000 claims abstract description 35
- 238000001354 calcination Methods 0.000 claims description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000002910 solid waste Substances 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims 1
- 229910052782 aluminium Inorganic materials 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 238000004321 preservation Methods 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 11
- 239000011148 porous material Substances 0.000 abstract description 10
- 238000001035 drying Methods 0.000 abstract description 8
- 239000002131 composite material Substances 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 7
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 239000005416 organic matter Substances 0.000 abstract description 3
- 238000004140 cleaning Methods 0.000 abstract description 2
- 238000003915 air pollution Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 7
- 238000005303 weighing Methods 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 4
- 229910052740 iodine Inorganic materials 0.000 description 4
- 239000011630 iodine Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 2
- 150000004056 anthraquinones Chemical class 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 239000007857 degradation product Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000005350 fused silica glass Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012229 microporous material Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
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Abstract
本发明涉及一种利用废弃活性氧化铝制备苯吸附材料的方法，它是将废活性氧化铝经清洗、过滤、干燥后，采用低温密闭热处理方式制备一种活性氧化铝/活性炭复合材料，对苯具有良好的吸附效果。本发明采用密闭低温热处理的方式，一方面可使废弃活性氧化铝被堵的内部孔洞打通；另一方面可使吸附在废弃活性氧化铝中的有机物直接分解炭化，并存于氧化铝孔洞中成为活性炭，减少空气污染。本方法工艺新颖，简单易行，变废为宝成本低，具有重要的环保性和经济价值。The invention relates to a method for preparing a benzene adsorption material by using waste activated alumina, which is to prepare a kind of activated alumina/activated carbon composite material by adopting a low-temperature airtight heat treatment method after cleaning, filtering and drying waste activated alumina. Has a good adsorption effect. The invention adopts the method of airtight low-temperature heat treatment. On the one hand, the blocked internal pores of the waste activated alumina can be opened; on the other hand, the organic matter adsorbed in the waste activated alumina can be directly decomposed and carbonized, and stored in the pores of the alumina to become activated carbon. ,reduce air pollution. The method is novel in technology, simple and easy to implement, low in cost for turning waste into treasure, and has important environmental protection and economic value.
Description
技术领域 technical field
本发明涉及一种废弃活性氧化铝的利用方法，具体为利用废弃活性氧化铝制备苯吸附材料的方法。 The invention relates to a method for utilizing waste activated alumina, in particular to a method for preparing a benzene adsorption material by using waste activated alumina.
背景技术 Background technique
随着工业的发展，世界各国工业催化剂的用量迅速增加，大部分废催化剂、废吸附剂作为固体废弃物丢弃，不仅造成资源浪费，也对环境造成极大的污染。活性氧化铝是催化剂载体和吸附剂的主要品种之一，它具有纯度高、原料易得、加工方便、物化性质可调等优点。在化工厂的双氧水工业生产中，活性氧化铝被用来吸附蒽醌降解物，也用来将这些降解物转化为有效蒽醌。随着使用时间的延长，氧化铝的活性会逐渐降低，直到不能满足生产要求而必须进行更换。更换下来的废弃活性氧化铝大量废弃，不仅造成了资源的浪费，散发出的臭气还会污染境造。 With the development of industry, the amount of industrial catalysts in various countries in the world has increased rapidly, and most of the spent catalysts and spent adsorbents are discarded as solid waste, which not only causes waste of resources, but also causes great pollution to the environment. Activated alumina is one of the main types of catalyst carrier and adsorbent, which has the advantages of high purity, easy access to raw materials, convenient processing, and adjustable physical and chemical properties. In the industrial production of hydrogen peroxide in chemical plants, activated alumina is used to adsorb anthraquinone degradation products and also to convert these degradation products into effective anthraquinones. With the prolongation of use time, the activity of alumina will gradually decrease until it cannot meet the production requirements and must be replaced. A large amount of replaced waste activated alumina is discarded, which not only causes a waste of resources, but also pollutes the environment with the odor emitted.
发明内容 Contents of the invention
本发明的目的是提供一种利用废弃活性氧化铝制备苯吸附材料的方法，本方法简单易行，成本低廉，二次污染少，有效利用了废弃资源，社会与经济效益显著。 The purpose of the present invention is to provide a method for preparing benzene adsorption material by using waste activated alumina. The method is simple and easy, low in cost, less in secondary pollution, effectively utilizes waste resources, and has remarkable social and economic benefits.
本发明的技术方案如下：将废活性氧化铝经清洗、烘干或晒干后，置于窑炉中300-600℃密闭煅烧，保温2~3h，然后自然冷却至室温，即制得苯吸附材料。 The technical scheme of the present invention is as follows: After cleaning, drying or sun-drying the waste activated alumina, put it in a kiln for 300-600°C closed calcining, keep it warm for 2-3 hours, and then cool it naturally to room temperature to obtain benzene adsorption Material.
所述的废活性氧化铝为化工厂双氧水生产过程中，用以净化和再生工作液的活性氧化铝，经使用失效后的颗粒状固体废弃物。 The waste activated alumina is the granular solid waste of the activated alumina used to purify and regenerate the working fluid in the hydrogen peroxide production process of the chemical plant after use.
本发明的效益和优越性在于：本发明以废弃活性氧化铝为原料，并针对废弃活性氧化铝中吸附有大量有机物的特点，采用简便的密闭低温煅烧的方法将有机物炭化，由于活性氧化铝已经是微孔材料，经炭化后的炭也达到微米级，自然形成一种活性氧化铝与活性炭的复合材料，研究实验表明，制得的复合材料对苯的吸附性能优异。 The benefit and superiority of the present invention are: the present invention uses waste activated alumina as raw material, and aiming at the characteristics that a large amount of organic matter is adsorbed in the waste activated alumina, adopts a simple method of airtight low-temperature calcination to carbonize the organic matter, because the activated alumina has already It is a microporous material. After carbonization, the carbon also reaches the micron level, and naturally forms a composite material of activated alumina and activated carbon. Research experiments show that the obtained composite material has excellent adsorption performance for benzene.
具体实施方式 Detailed ways
原料：废弃活性氧化铝。 Raw material: waste activated alumina.
具体制备步骤为： Concrete preparation steps are:
（1）预处理：将废弃活性氧化铝用清水漂洗去除杂质，放入干燥箱中烘干或晒干。 (1) Pretreatment: Rinse the waste activated alumina with clean water to remove impurities, and put it in a drying oven to dry or dry in the sun.
（2）煅烧：将烘干好的废弃活性氧化铝装入密闭容器中，盖好盖子，放入窑炉，进行低温热处理（以200℃/h的升温速率升至300-600℃，保温2~3h），炭化处理后自然冷却，即可。附：苯吸附测定与计算方法 (2) Calcination: Put the dried waste activated alumina into an airtight container, cover it, put it into a kiln, and perform low-temperature heat treatment (raise the temperature to 300-600°C at a rate of 200°C/h, keep it for 2 ~3h), after carbonization treatment, cool naturally. Attachment: Benzene adsorption measurement and calculation method
采用密闭的玻璃干燥器，在干燥器的底部倒入液体苯，将事先称好的试样装入称量瓶中称量，试样重为m0，总重为m1，然后将打开盖子的称量瓶放在干燥器的隔板上，盖好干燥器的盖子。在恒定温度30℃下，苯自然挥发，吸附24h，吸附结束后，取出称量瓶并快速盖上盖子后称量，记吸附后总重为m2，采用下式计算苯吸附率。 Use a closed glass desiccator, pour liquid benzene into the bottom of the desiccator, put the pre-weighed sample into a weighing bottle and weigh it, the sample weight is m 0 , the total weight is m 1 , and then the lid is opened The weighing bottle is placed on the partition of the desiccator, and the lid of the desiccator is closed. At a constant temperature of 30°C, benzene is naturally volatilized and adsorbed for 24 hours. After the adsorption is completed, take out the weighing bottle and quickly cover it and weigh it. Record the total weight after adsorption as m 2 , and use the following formula to calculate the benzene adsorption rate.
式中：η—试样的苯吸附率，%； In the formula: η —the benzene adsorption rate of the sample, %;
m 0 —试样和称量瓶总重，g； m 0 —the total weight of sample and weighing bottle, g;
m 1 —未吸附干燥后试样和称量瓶总重，g； m 1 - the total weight of the sample and the weighing bottle after no adsorption drying, g;
m 2 —吸附后试样和称量瓶总重，g。 m 2 —the total weight of sample and weighing bottle after adsorption, g.
下面结合具体实施例对本发明内容进行具体说明： Below in conjunction with specific embodiment content of the present invention is specifically described:
实施例1： Example 1:
利用废弃活性氧化铝研制苯吸附材料，其原料如下：废弃活性氧化铝。 The benzene adsorption material was developed by using waste activated alumina, and its raw materials were as follows: waste activated alumina.
制备步骤为： The preparation steps are:
（1）预处理：将废弃活性氧化铝经清水洗涤，晒干。 (1) Pretreatment: Wash the waste activated alumina with water and dry it in the sun.
（2）煅烧：将烘干好的废弃活性氧化铝装入陶瓷坩埚中，盖好盖子，放入窑炉，以200℃/h的升温速率升至300℃保温3h，随炉冷却后即得复合材料。 (2) Calcination: Put the dried waste activated alumina into a ceramic crucible, cover the lid, put it into the kiln, raise the temperature to 300°C at a rate of 200°C/h and keep it for 3 hours, then cool down with the furnace to get composite material.
性能：试样的碘吸附值为233.27 mg/g、试样的炭元素含量为3.57%，比表面积为234.70m2/g、孔容为0.41m3/g、平均孔径为6.59 nm，试样对苯具有良好的吸附效果，饱和吸附率可达21.80%。 Performance: The iodine adsorption value of the sample is 233.27 mg/g, the carbon element content of the sample is 3.57%, the specific surface area is 234.70m 2 /g, the pore volume is 0.41m 3 /g, and the average pore diameter is 6.59 nm. It has a good adsorption effect on benzene, and the saturated adsorption rate can reach 21.80%.
实施例2： Example 2:
利用废弃活性氧化铝研制苯吸附材料，其原料如下：废弃活性氧化铝。 The benzene adsorption material was developed by using waste activated alumina, and its raw materials were as follows: waste activated alumina.
制备步骤为： The preparation steps are:
（1）预处理：将废弃活性氧化铝经清水洗涤，放入干燥箱中恒温100℃烘干1h。 (1) Pretreatment: Wash the waste activated alumina with clean water, put it in a drying oven at a constant temperature of 100°C and dry it for 1 hour.
（2）煅烧：将烘干好的废弃活性氧化铝装入不锈钢罐子中，盖好盖子，放入窑炉，以200℃/h的升温速率升至400℃保温2h，随炉冷却后即得复合材料。 (2) Calcination: Put the dried waste activated alumina into a stainless steel jar, cover the lid, put it into the kiln, raise the temperature to 400°C at a rate of 200°C/h and keep it for 2 hours, then cool it down with the furnace. composite material.
性能：试样的碘吸附值为231.44 mg/g、炭元素含量为2.36%，比表面积为205.1m2/g、孔容为0.43m3/g、平均孔径为7.82nm，试样对苯具有良好的吸附效果，饱和吸附率可达23.28%。 Properties: The iodine adsorption value of the sample is 231.44 mg/g, the carbon element content is 2.36%, the specific surface area is 205.1m 2 /g, the pore volume is 0.43m 3 /g, the average pore diameter is 7.82nm, the sample has a Good adsorption effect, the saturation adsorption rate can reach 23.28%.
实施例3： Example 3:
利用废弃活性氧化铝研制苯吸附材料，其原料如下：废弃活性氧化铝。 The benzene adsorption material was developed by using waste activated alumina, and its raw materials were as follows: waste activated alumina.
制备步骤为： The preparation steps are:
（1）预处理：将废弃活性氧化铝经清水洗涤，放入干燥箱中恒温100℃烘干1h。 (1) Pretreatment: Wash the waste activated alumina with clean water, put it in a drying oven at a constant temperature of 100°C and dry it for 1 hour.
（2）煅烧：将烘干好的废弃活性氧化铝装入不锈钢罐子中，盖好盖子，放入窑炉，以200℃/h的升温速率升至500℃保温2h，随炉冷却后即得复合材料。 (2) Calcination: Put the dried waste activated alumina into a stainless steel jar, cover the lid, put it into the kiln, raise the temperature at a rate of 200°C/h to 500°C and keep it for 2 hours, and then cool it down with the furnace. composite material.
性能：试样的碘吸附值为231.44mg/g、炭元素含量为1.89%，比表面积为242.20m2/g、孔容为0.46m3/g、平均孔径为7.11 nm，试样对苯具有良好的吸附效果，饱和吸附率可达24.01%。 Performance: The iodine adsorption value of the sample is 231.44mg/g, the carbon element content is 1.89%, the specific surface area is 242.20m 2 /g, the pore volume is 0.46m 3 /g, the average pore diameter is 7.11 nm, the sample has a Good adsorption effect, the saturation adsorption rate can reach 24.01%.
实施例4： Example 4:
利用废弃活性氧化铝研制苯吸附材料，其原料如下：废弃活性氧化铝。 The benzene adsorption material was developed by using waste activated alumina, and its raw materials were as follows: waste activated alumina.
制备步骤为： The preparation steps are:
（1）预处理：将废弃活性氧化铝经清水洗涤，放入干燥箱中恒温100℃烘干1h。 (1) Pretreatment: Wash the waste activated alumina with clean water, put it in a drying oven at a constant temperature of 100°C and dry it for 1 hour.
（2）煅烧：将烘干好的废弃活性氧化铝装入熔融石英质坩埚中，盖好盖子，放入窑炉，以200℃/h的升温速率升至600℃保温2h，随炉冷却后即得复合材料。 (2) Calcination: Put the dried waste activated alumina into a fused silica crucible, cover the lid, put it into the kiln, raise the temperature at a rate of 200°C/h to 600°C for 2 hours, and cool it with the furnace A composite material is obtained.
性能：试样的碘吸附值为232.36mg/g、炭元素含量为2.03%，比表面积为237.2m2/g、孔容为0.47m3/g、平均孔径为7.58 nm，试样对苯具有良好的吸附效果，饱和吸附率可达24.19%。 Performance: The iodine adsorption value of the sample is 232.36mg/g, the carbon element content is 2.03%, the specific surface area is 237.2m 2 /g, the pore volume is 0.47m 3 /g, the average pore diameter is 7.58 nm, the sample has Good adsorption effect, the saturation adsorption rate can reach 24.19%.
由以上实施里可以看出本方法制备的苯吸附材料对苯的吸附效果良好，饱和吸附值均可达到20%以上。 From the above implementation, it can be seen that the benzene adsorption material prepared by this method has a good adsorption effect on benzene, and the saturated adsorption value can reach more than 20%.
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